PB84-223023
     Causes of Papillosr.as  on  Pish Exposed to
     Chlorinated Sewage Effluent
     Auburn Univ., AL
     Prepared for

     Environmental Research Lab., Gulf Breeze,  FL
    Jul  84

                                    '^3
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                                            EPA-600/3-84-076
                                                 1984
      CAUSES OF PAPILLOMAS ON FISH EXPOSED
         TO CHLORINATED SEWAGE EFFLUENT
                       by

        John M. Grizzle and Paul Melius
Department of Fisheries and Allied Aquacultures
          and Department of Chemistry
       Auburn. University, Alabama  36849
                  CR809336010
                Project Officer

                 William Davis
       Environmental Research Laboratory
          Gulf Breeze, Florida  32561
       ENVIRONMENTAL RESEARCH LABORATORY
       OFFICE OF RESEARCH AND DEVELOPMENT
      U.S. ENVIRONMENTAL PROTECTION AGENCY
          GULF BREEZE, FLORIDA  32561

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                                   TECHNICAL REPORT DATA
                            (Please read Instnuti^ni on the reverse before completing}
 . REPORT NO.
   EPA-6GO/3-84-076
             3. RECIPIENT'S ACCESSION NO.
                  PS83  223023
4. TITLE AND SUBTITLE
  CAUSES OF PAPILLOMAS ON  FISH  EXPOSED TO CHLORINATED
  SEWAGE EFFLUENT
             5. REPORT DATE
               July  1934
             6. PERFORMING ORGANIZATION CODE
7. AUTHORS)
  J.M.  Grizzle and Paul Melius
                                                            I. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
                                                            tO. PROGRAM ELEMENT NO.
 Department of Fisheries and Allied Aquacultures &
 Department of Chemistry
 Auburn University, Alabama 36849
             11. CONTRACT/GRANT NO.
             CR80933010
12. SPONSORING AGENCY NAME AND ADDRESS
 U.S.  Environmental Protection Agency
 Environmental  Research Laboratory
 Office  of Research & Development
 Gulf  Breeze,  FL 32561
                                                            13. TYPE OF REPORT AND PERIOD COVERED
             14. SPONSORING AGENCY CODE
                EPA/600/04
IS. SUPPLEMENTARY NOTES

16. ABSTRACT.
          This research was initiated to determine the cause  of oral  papillomas in
     black bullheads (Ictalurus  melas) from the final oxidation pond  of the
     Tuskegee, Alabama, sewage treatment plant.  The water  in this pond was
     chlorinated effluent from the  sewage treatment plant.
          The presence of a carcinogenic and mutagenic chemical  in the effluent of a
     sewage treatment plant was  indicated by papillomas developing on caged black
     bullheads, glucuronosyl transferase induction in caged  channel catfish, and
     Ames-test mutagenicity of water extract.  Unlike previously studied fish
     papillomas, virus-like particles were not present in the  tumor cells.  Although
     mutagenic and carcinogenic  chemicals have not been identified in the
     wastewater, chlorine is  implicated as a factor contriubting to the induction of
     the  papillomas because the  prevalence of papillomas on wild black bullheads
     exposed to the effluent  decreased from 73% to. 23% after  the dtlorination rate
     was  reduced.
          This report was submitted in fulfillment of Grant No.  LCR8Q9336010 by
     Auburn University under  the sponsorship of the U.S. Environmental Protection
     Agency.  This report covers the period from 12 October 1981 to 11 October 1983,
     and  work was  completed as of 11 October 1983.
17.
                                KEY WORDS AND DOCUMENT ANALYSIS
                  DESCRIPTORS
                                              b.IDENTIFIERS-OPEN ENDED7SRMS  C.  COSATI Field/Group
18. DISTP.iSUTSON STATEMENT


   Release  to  public
19. SECURITv_<-^r.35 • /Viu Kep
  unclassified
21. .N'Q. OF PAGES

       33.
20. SECURITY CLASS , rtlii pJtt
                           22.
EPA Form 2220-1 (Rev. 4-77)   PREVIOUS EOITION >s

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                      NOTICE

This document has been reviewed in accordance with
U.S. Environmental Protection Agency policy and
approved for publication.  Mention of trade names
or commercial products does not constitute endorse-
ment or recommendation for use.
                       11

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                                    FOREWORD

     The protection of our estuarine and coastal  areas  from damage  caused by
toxic organic pollutants requires that regulations restricting the  introduction
of these compounds into the environment be formulated  on  a  sound  scientific
basis.  Accurate information describing dose-response  relationships  for organisms
and ecosystems under varying -conditions is required.   The EPA  Environmental
Research Laboratory, Gulf Breeze, contributes to this  information through
research programs aimed at determining:

     the effects of toxic organic pollutants on individual  species  and
     communities of organisms;

     the effects of toxic organics on ecosystem processes and  components;

     the significance of chemical carcinogens in the estuarine and  marine
     environments.

     Few studies have reported carcinogenic expressions in  populations of
fishes, and still fewer researchers have been able to  manipulate  the frequency
of the tumor expression.  In this report, a population  of catfish exposed to
chlorinated sewage effluent are caged and compared with related species, and
efforts to separate the tumor inducer were undertaken.   Results indicated that
the incidence of papillomas declined after the chlorination rate  was reduced.
These data provide an intriguing link between waste water treatment  and tumor
induction in fish.
                                                 Enos
                                        Director
                                        Environmental Research Laboratory
                                        Gulf Breeze,  Florida
                                      TM

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                                    ABSTRACT
     This research aas initiated  to  determine  the cause  of  oral  papillomas  in''
black bullheads (Ictalurus melas)  from  the  final oxidation  pond  of  the  Tuakegee,
Alabama, sewage treatment plant.   The water in this  pond was  chlorinated  efflu-
ent from the sewage treatment plant.

     The presence of a carcinogenic  and mutagenic chemical .in the effluent  of  a
sewage treatment plant was indicated by papillomas developing on caged  black
bullheads, glucuronosyltransferase induction in caged  channel catfish,  and
Ames-test mutagenicity or water extract.  Unlike previously studied fish
papillomas, virua-like particles were not piresent in. the tumor cells.   Although
mutagenic and carcinogenic chemicals have not  been identified in the wastewater,
chlorine is implicated as a  factor contributing to the induction of the
papillomas because the prevalence  of papillomas on wild  black bullheads exposed
to the effluent decreased from 73% to 23% after- the  chlorination rate was
reduced.  .
          \                               ./
     This report was subsitted in  fulfillment  of Grant No.  CR80933&010  by Auburn
University under the sponsorship  of  the U.S. Environmental  Protection. Agency.
This report covers the period from 12 October  1981 to  11 October 1983,  and  work
was completed as of 11 October 1983.
                                        IV

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                                    CONTENTS

                                                                          Page

Abstract	     iv

Figures	  .	     vi

Tables	    vii

Acknowledgments   ....'	viii

   1.  Introduction   	      1
   2.  Conclusions and Recommendations  .  	      2
   3.  Study Site	      3
   4.  Materials  and  Methods  .	      6
   5.  Results	     10
   6.  Discussion	     19

References	     21

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                                    FIGURES


Number                                                                     Page

  1  Schematic plan of Che Tuskegee, Alabama, sewage treatment plant  ...   4


  2  Total residual chlorine (monthly averages)  in water leaving the
    . chlorine contact chamber of the Tuskegee sewage treatment plant   .  .    5

  3  Prevalence of papillotnas on wild black bullheads from the final
     oxidation pond of the Tuskegee sewage treatment plant   . .  	    11

  4  Oral papillcina on the mouth fornix of a black bullhead.                 12

  5  Superficial portion of an oraL papilloma.   Epithelial cells,
     goblet cells, and alarm substance cells are arranged around
     lumens forming cell nests	.	    13

  6  Response of Salmonella typhimurium strain TA100 in the  Ames test
     to organic extracts of water collected at the inlet or  outlet of
     the final oxidation pond of the Tuskegee, Alabama, sewage treatment
     plant	    16

  7  UDP-glucuronosyltransferase activity (nmol/min/ng protein)in
     liver microsomes of caged channel catfish in the final  oxidation
     pond of the Tuskegee, Alabama, sewage treatment plant or in a
     control pond	    16
                                       VI

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                                      TABLES
Number
     Maximum prevalence of oral  lesions  on  caged  fish  in the  final
     oxidation pond of the Tuskegee  sewage  treatment plant  ....
                                       VII

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                                ACKNOWLEDGMENTS
     The cooperation of the South Tuskegee Water Pollution Control Plant
personnel, is gratefully acknowledged.  Auburn University staff and graduate
students that contributed to this project were Barrie Tan, Chalor Limsuwan,
Leonard Hochstedler, Paraskevi Karathanasis, Diane Biba, Richard Maxwell, Jai
Hosey, and Steve Horowitz.
                                      Vlll

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                                   SECTION 1

                                  INTRODUCTION
     A population of black bullheads in the final oxidation pond of the City of
Tuskegee, Alabama, sewage treatment plant had a 73% prevalence of oral
papillomas (Grizzle et al. 1981).  These fish provided an opportunity to study
the cause of fish papillomas, especially as related to chlorinated sewage
effluent.

     Sewage entering this treatment plant did not include discharge from
industries or institutions, but run-off water from residential and agricultural
areas entered the plant after rains.  The process of chlorinating the sewage
after it passed through an aeration basin and a settling basin was considered a
possible source of carcinogens.

     There has been only one previous report of a high prevalence of neoplasms
in aquatic animals living in chlorinated sewage effluent (Rose 1977).  In that
case, a pond at Reese Air Force Base, Texas, contained tiger  salamanders
(Ambystoma tigrinum) that had neoplastic and non-neoplastic lesions with a peak
frequency of 53%.  Chemical carcinogens, especially perylene, were suspected of
causing the lesions.

     Papillomas occur on many species of fish and have been associated with
pollution (Lucke and Schlumberger  1941; Russell and Kotin 1957; Cooper and
Keller 1969; Sonstegard 1977; Dawe and Harshbarger 1975) and  tumorogenic viruses
(Edwards et al. 1977; Schwanz-Pfitzner 1976; McAllister et al. 1977).  Other
fish tumors have a genetic origin  (Siciliano et al. 1971; Vielkind et al. 1971).

     Laboratory and field experiments were  initiated to determine the cause of
the papillomas.  Some of these experiments  were a continuation of a previous EPA
cooperative agreement (CR807844010, Grizzle and Melius 1983).  Objectives were
to:  (1) determine the prevalence  of papillomas on fish in the final oxidation
pond; (2) describe the histology and ultrastructure of the papillomas; (3)
determine if the papillomas would  persist on black bullheads  taken from  the
final oxidation pond and placed in clean water; (4) chemically identify
mutagenic and carcinogenic chemicals in the water; (5) determine  if the  water
was mutagenic; (6) determine if tumors would develop in new fish  placed  intc the
final oxidation pond; (7) determine if hepatic-enzyme induction occurred in fish
exposure to the water (8)- determine if viruses were associated with the
papillomas by ultrastructural examination,  transmission by cell-free homogenate,
and isolation of virus wLth cell-culture techniques; (9) determine if lesion?
would develop in brown bullheads exposed during embryonic development to a
concentrate of the final oxidation pond water; and (10) determine if tumors
would develop on black bullheads exposed to an organic concentrate of the final
oxidation pond sediment injected or applied topically to che  mouth.

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                                   SECTION 2

                        CONCLUSIONS AMD RECOMMENDATIONS
     The Tuskegee, Alabama, sewage  treatment plant  final oxidation pond had
wild black bullheads with a 73% prevalence of oral  papillomaa.   Results of this
study indicated that the acidic organic,  solvent extract of  this  oxidation pond
water was seasonally cucagenic to Salmonella typhimurium bacterial tester
strains TA98 and TA100 if activated with Arochlor-induced rat  liver  enzymes.  No
evidence of a viral etiology  for the  papillonas was found during ultraatructural
studies of the lesions or during transmission attempts.
                                             V
     Caged black bullheads in the oxidation pond developed  oral  papillomae in
the saraa mouth location occupied by papilloraas in wild black bullheads.  The
lesions in caged fish were probably related to the  mutagenic chemicals in the
water because there was also  induction of hepatic enzymes in fish exposed to the
final oxidation pond water.   Neoplasms did not.develop in adult  fiah or embryos
exposed to water or sediment  extracts.      ••'
                                                     ^
     The usefulness of exposing caged fish to water for detection of chemical
carcinogens was demonstrated  by the development -of  neoplasms on  caged black
bullheads.  The use of chemical analysis in this case  failed to  indicate that
rautagenic or carcinogenic chemicals were present.   Laboratory  exposures of black
bullheads and brown bullhead  embryos  to  organic extracts of the  Tuskegee
wastewater failed to cause tumors.  Additional refinement of techniques may
improve the usefulness of laboratory  exposures, but. presently  field  exposures  .
of caged fish are more conclusive.

     Chlorination was implicated in the  induction of the papillomas  because  the
prevalence decreased after the chlorination rate was reduced.  Further studies
should determine the identity of the  rautagenic .and  carcinogenic  chemicals, the
role of chlorine in causing these tumors, and the persistence  of the
carcinogenic chemicals after  release  into the receiving stream.

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                                   SECTION 3

                                   STUDY SITE
     The 0.8-ha final oxidation pond of the Tuskegee, Alabama, sewage treatment
plant was designed for post-secondary treatment of sewage effluent.  Water
retention time in the pond depends on the flow rate and averages 4-5 days.
Sewage treatment before the oxidation pond consists of sedimentation, activated
sludge secondary treatment, and disinfection by cholorination (Fig. 1).  During
January-November 1979, monthly average residual chlorine concentration was
1.2-3.1 mg/liter in the effluent leaving the chlorine contact chamber and when
entering the final oxidation pond (Fig. 2).  Since November 1979 this chlorine
concentration has ranged from 0.3 to 1.2 mg/liter.  Residual chlorine
concentration of water leaving the final oxidation pond is usually.0.1 mg/liter,
approximately the same as before November 1979.

     The- portion of Tuskegee's sewage that entered this plant contained only
domestic wastes; however, following heavy rainfall the flow rate into the plant
increased greatly, indicating that surface runoff  from surrounding agricultural
and residential areas entered the sewage system.

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                  B
                                t
                             4  ~l
                                  a
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FIGURE 1. Schematic plan of the Tuskegee, Alabama, sewage treatmsat plant.  A,
pumping station; B, grit removal; C, aeration basins; D,  settling basins; E,
chlorine contact chamber; F, final oxidation .poad4

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FIGURE 2.  Monr.aly averages  for  total  residual chlorine (mg/liter) in water
leaving -the chlorine cotact  of the  Tuskegee sewage treatment plant.

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                                   SECTION 4

                             MATERIALS AND METHODS
     Fish were collected  from  the  final  oxidation  pond  of  the Tuskegee,  Alabama.
sewage treatment plant with gill nets  and  traps.   During 2 bacterial epizootics,
moribund fish were picked up with  a  dip  net.   For  determining prevalence of
papillomas, most papilloaaa were diagnosed grossly.   Representative  lesions were
examined by light microscopy to confirm  the diagnosis.  Fish were  put  back into
the pond if they were not necropsied or  used  in experiments.  The  papillomas  on
26 adult black bullheads  from  the  final  oxidation  pond  were measured,  the fish
were identified with tags, and then  placed in 3-m  diameter plastic pools at the
Alabama Agricultural Experiment Station, Auburn, Alabama,  to determine the fate
of papillomas after the fish were  placed in clean  water.

     .For light microscopy, tissues were  fixed in 10%  buffered formalin or
Bouin's, embedded in paraffin, sectioned at 6-inn thickness, and  stained  with
hematoxylin and eosin.  Selected paraffin  sections were also stained with
periodic acid-Schiff, Masson's trichrome stain, and Feulge^ reaction.

     For transmission electron microscopy  (TEM), 1-mnr'  pieces of tissue  fixed
in phosphate buffered glutaraldehyde and post-fixed in  osmium tetroxide  were
embedded in Eopn-Araldite, sectioned at  approximately 70-raa thickness, and
stained with lead citrate and uranyl acetate.

     The Alabama Pesticide Residue Laboratory, Auburn,  Alabama,  and  the  Alabama
Department of Public Health Laboratory,  Montgomery, Alabama, used  gas
chromatography to determine if toxic organic  chemicals  were in  the water or
sediment of the final oxidation pond.

     Extracts of the final oxidation pond  water were  tested for  mutagenicity
with the Ames test (Ames  et al. 1975)  using Salmonella  .typhmurium tester
strains TA 98 and TA 100  supplied  by Dr. Anie!~IPositive controls  were run with
benzo(a)pyrene.  Three types of organic  extracts of the pond water
for mutagenicity testing.  For one procedure  10 liters  water was filtered
through XAD resin and the organics were  eluted with acetone.  For  the  other
procedures,   the pH of 2 liters of  water  was adjusted  to  either 1.0 with HC1
(for acid fraction) or 12-13 with  NaOH (for basic  fraction) and  then extracted
three times with 200 ml of 25% ether and 75%  hexane per liter of water.   For  all
procedures, the bulk of the solvents were  removed  by  distillation.  The  last  20
ml of solvent was evaporated under a stream of nitrogen.   Extracts were
dissolved in dimethylsulfoxide and filter  sterilized  before addition to  the
agar.  Concentration of the organic  extract ranged from 0.3-3.0  mg/plate.

     Black bullheads, brown bullheads  (Ictalurus nebuloaus), yellow  bullheads
(Ictalurus natalis), and  channel catfish (IctalTTrus punctatus) were  placed into
cagesInthefinal oxidation pond  and  a  controlpond  atthe Alabama  Agricultural
Experiment Station.  The  1-m  cages  were allowed to rest on the  pond bottom
(sinking cages) or suspended off the bottom by floats (floating  cages).   Cages
were placed at three locations in  the  final oxidation pond:  near  the  inlet
(inlet A), approximately  60 meters from  the inlet  (inlet B) or near  the  pond

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outlet (outlet).  Most cages were stocked with 50 fish of a single species with
total lengths of the fish between 5-10 en. .

     Glucuronosyltransferase (CDP-GT) and sulfotransferase (ST) were assayed in
livers of caged fish as part of a separate- EPA cooperative agreement to Dr. D.
R. Strength (Department of Animal and Dairy Sciences, Auburn University). .
Livers were homogenized in a Potter-Elvehjem-type homogenizer with teflon pestle
with 4 parts of 0.25 sucrose containing 0.01M Tris, pH 7.5.  A clarified
hotnogenate was prepared by centrifuging at lO.OOOxg for 30 min.  Microsomes were
sedimented at iOO.OCOxg for 1 hr, yielding the supernate and microsomal
fractions.  The microsomes were washed twice in Tris-sucrose buffer, recovered
by centrifugation and suspended in 0.1M Tris buffer, pH 7.5 prior to use or
storage.  Supernate fractions for immediate assay of ST were prepared by
homogenizing livers directly in 0.1M Tris buffer, pH 7.5, and centrifuging 1 hr
at lOO.OOOxg.  Protein concentrations were determined by the procedure of Lowry
et al. (1951).
                                         V
     UDP-GT was assayed colorimetrically by the decrease in absorbance at 400 run
using p-nitrophenol as ar. acceptor.  The reaction ixture contained the following
in umoles;  p-nitrophenol, 0.12; UDP-glucuronic acid, 1.2; MgC^. 4; Tris
buffer, pH 7.5, 11; the total reaction volume of 0.2 ml also contained 40 ug of
Triton X-100 and 20 to 50 ug of microsomal protein.  The reaction was started by
adding UDPGA and stopped after 10 min incubation at 37 C by adding 0.2 ml of
ethanol.  The reaction mixture was then centrifuged for 10 min at l.OOOxg and
0.1 ml of the supernate was added to 0.9 ml of 0.1M EDTA, pH 9.6 and the
AAQO determined.  The change in absorbance was determined from the
difference in A4QQ of identical reaction mixtures incubated zero and 10
min, respectively; the quantity of p-nitrophenol was ascertained from standard
solutions measured in the same medium.
                                          t
     ST activity was determined colorimetrically measuring the p-nitrophenol
released from PNPS in the presence of PAP.  The reaction mixture from the
lOO.OOOxg supernate fraction of tissues in a total volume of 1.0 ml.  The
reaction was conducted at 37 C for 10 min and was terminated by adding 2.5 ml of
ethanol.  After centrifugation at lOOOxg for 10 min, the supernate was decanted
into a tube containing 0.5 ml of 0.2M glycine buffer, pH 10.4 and i nil of
distilled water (total volume used 5 ml).  The absorbance at 400 rim was measured
in a spectrophotometer, or alternatively in a Klett-Summerson Colorimeter with
#42 filter.  Zero time controls and standard solutions of p-nitrophenol were
measured in similar fixtures; the p-nitrohenol libertated from PNPS was      ;
expressed in nmoles/min/mg protein.

     Papillomas from final oxidation pond black bullheads were homogenized  in
Hank's.balance salt solution (HBSS), filtered.through a 0.45-um  filter, and  .
injected subcutaneously into the mouth fornices of 19 adult black bullheads.'
Seven control black bullheads were injected with HBSS.  Each fish was kept  in a.
separate 40-liter aquarium and examined monthly.

     Brown bullhead broodstock were obtained from Easterling's Fish Hatchery,
Clio, Alabama.  On May 18, 1981, paired broodfish were placed in spawning pens
in an earthen pond at the Alabama Agricultural Experiment Station.  Spawning
boxes were checked for eggs twice daily and egg-s were transferred to
recirulating aquaria.                        •     '

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     Eggs wer» kept  in  a  recirculating  systems  with 10,  15-liter aquaria.
Filtered pond water  was used  to  fill  the  system initially aud to replace water
lost by leakage.  Water drained  from  the  aerated aquaria into a lower,  273-liter
reservoir and then flowed by  gravity  to the  aquaria.  Eggs ware incubated in a
recirculating system instead  of  the customary,  flow-through troughs to  avoid the
use of pond water with  variable  water quality.

     Aqueous solutions  of afltoxin Bj (AFB)  were prepared from a 500 rag/liter
stock solution.  To  facilitate solubilization,  10 mg AFB (Sigma Co., St. Louis,
Mo.) were dissolved  in  10 ml  divnethylsulfoxide  (DM50) and ethanol.   Aflatoxin
Bi was not purified  prior to  use.  DMSO was  added/as a solvent after it was
observed that ethanol alone was  insufficient for Solubilization.  Aflatoxin Bj
concentrations of 0.5,  1.0 and 1.5 Qg/liter  were made from the stock solution
with reconstituted soft water immediately before use.

     Organic compounds  were extracted from 15 liters of water collected at the
outlet from the  final oxidation  pond  of the  South Tuskegee Water Pollution
Control Plant, Macon County,  Alabama, in  mid-May 1981.  The extraction
procedure, a modification of  the technique used by Rappaport et al. (1979), used
a column of purified XAD-2 end XAD-7  resin.   Unfiltered water flowed into the
column by gravity at 19 ml/miu.   The  column was dried under nitrogen to remove
residual water,  and  prganics  were eluted  with acetone.  The acetone was then
dried under a nitrogen  stream and the flask containing dried organics was stored
at -20 C.

     Prior to embryo exposure, the yellowish-brown film of organics was
redissolved i.i 0.2-ml 95% ethanol and 0.4-ml DMSO,  and diluted to 200 ml with
.reconstituted soft water. The final, 200-nil solution was a 75-fold -concentrata
of the effluent-water organics.   Organic  yield  was not directly measured but
estimated to be  between 0.7 mg/liter  and  1.0 ing/liter (10 and 15 mg for 15
liters) based on later  extractions of the same  water.

     When eggs.were  five  days of age, the egg mass was subdivided into  groups of
approximately 200 eggs, and each group  was placed in 300-ml glass dishes
containing 200 ml of the  sublethal test solutions for one hour.

     After hatching,  fish were kept in  aquaria  until the yolk sac was absorbed.
Fish from the first  replicate were transferred  to 5700-liter plastic pools and
fish from the second replicate were kept  by treatment group in cages in an
earthen pond on  the  Alabama Agricultural  Experiment Station.  Fry were  fed on a
48% crude protein diet  (Silver Cup No.  1), and  after four months of age on a 36%
crude protein feed (Auburn Feed  No. 3).

     The only treatments  sampled from the first replicate were the 0.5  mg/liter
AFB and solvent  control,  due  to  accidental drainage of the other plastic pools
after stocking.  Samples  of three to  five fish  from the two treatments  surviving
in plastic pools were fixed in Bouin's  fluid daily for two weeks after
fertilization, and at 25  days, three  months, and six Lionths after hatching.
Samples of solvent control fish  were  fixed in Bouin's at these time periods for
histological examination  of normal liver  development and morphology.  Eight
months after hatching,  equal  numbers  of both the 0.5 mg/liter AFB and the
solvent control  treatments were  sampled as follows:  147 fixed in Bouin's, three

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dissected for fixation of livers  for  electron microscopy,  and  20 were held  for
tnicrosomal preparation of liver tissue.

     All but two treatments of the  second  replicate,  placed  in cages, were  lost
to bacterial infections during the  induction period.   Surviving treatments  were
the 1.0 mg/liter AFB group and the  Tuskegee effluent  concentrate group.   Brown
bullheads of the 1.0 mg/litcr AFB treatment were  fixed in  Bouin's  at 25  days
(four) and at eight months (twelve) after  hatching.   Four  brown bullheads
exposed to the Tuskegee effluent  concentrate were  fixed  in Bouin's 25 days  after
hatching.  Remaining fish cf the  effluent  concentrate treatment were later  lost
to bacterial infections.

     Sediment from the inlet area was collected and allowed  to dry for 96 hours.
The sediment was then further desiccated with Na2S04.  Organics from the
sediment were then extracted using  acetone and methylene chloride. The  extract
obtained after distillation was dissolved  in DMSO.  Six fish were  injected  in
the right mouth fornix with 0.1 ml  of the  extract  at  a concentration of  83.3
mg/ml DMSO.  Six control  fish received an  injection of 0.1 ral  DMSO.  Fish were
injected once every 2 months for  a  period  of 9 months.  The  same extract was
also dissolved with DMSO  to give  a  concentration  of 50 ng/ral DMSO. The  mixture
was-applied to the entire oral area of 8 black bullheads using a cotton  swab.
Each fish was swabbed with a circular motion for  1 minute, at  weekly intervale,
for a period of 6 months.  Eight  other fish that  served as controls received
weekly, 1-minute swabs of DMSO only.

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                                    SECTION  5

                                     RESULTS


PAPILLOMAS ON WILD BLACK  BULLHEADS  IN  THE FINAL OXIDATION POND

     The prevalence of papillomas in wild,  adult black bullheads  in  the  final
oxidation pond decreased  from  73% in 1980 to 23% in March 1983 (Fig.  3).
Another change in the papillomas was the size;  the  large  papillomas  seen
protruding from  the mouth of black  bullheads in 1979-1980 (Grizzle et al.  1981)
were not found in recent  samples.   All neoplasms were  located  in  the  oral  cavity
or on the lips except for 1 papilloma  and"*! dermal • fibroma on  the dorsal surface
of the heads of  2 specimens.

     The only other species of fish present in  the  final  oxidation pond  before
May 1980 were green sunfish (Lepomis cyanellus) and golden shiners (Notemigonus
crysoleucas).  During May and  July  1980, 2,000  silver  carp (Hypophthalmichtihys
molitrix) were released in the final oxidation  pond.  No  tumors were  found on
any of these species.                             s

     The papillomas consisted  of hyperplastic nucosa covering  papillae of
submucosa (Fig.  4).  Goblet cells and  alarm substance  cells were  absent  from
parts of the lesion; in other  areas these iells were numerous  and formed cell
nests (Fig. 5).  Cytoplasmic inclusion bodies in cells near the tumor surface
were eosinophilic, PAS positive, and weakly Feulgen positive.   The number  of
mitotic figures  was similar to that in normal oral  mucosa.

     Ultrastructurally, the oral papillomas of  wild black bullheads  from the
final oxiaation  pond had  epithelial cells resembling normal oral  mucosa  cells
and a central connective  tissue column that was continuous wit'n the  submucosa.
Near the tumor surface there were mucous cells, and plasma membranes  of  the
epithelial cells adhered  closely with  those of-adjacent cells.  Desmosomes
occurred less frequently  between the cells  than in  normal mucosa. Mitochondria,
endoplasimic reticulum, and ribosorces  wee concentrated in the  peripheral
cytoplasm of the epithlial cells.   These surface cells often contained glycogan
particles among  !.he tonofilamer.ts.   The mid to  near basal portion of  the
papilloma consisted of stellate epithelial  cells having more tonofilaments,
fewer organelles in the cytoplasm,  and more intercellular space than  epithelial
cells near the surface.   Desmosomes occurred more frequently between  the cells
in the basal area than near the. surface.  Alarm substances occurred  in the mid
portion of the epithelium and  were  surrounded by stellate cells.  Numerous
lymphocytes were present  in the basal  region of-the tumor.  The basal epithelial
cells contained  numerous  mitochondria, endoplasmic'reticulum,  and ribosomes in
the cytoplasm.   Plasma membranes adhered to the adjacent  cells by desmosomes.
Intercellular spaces occurred  less  frequently in the basal region than in  the
middle\portion of the tumor.             * «•  •
                                       10

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                                               0
              Jan 80 Jul 80 Jan 81  Jul 81  Jan 82 Jut 82  Jan 83  Jul 83
                                     DATE
FIGURE 3.  Prevalence of papillomas on wild black bullheads  from the  final
oxidation pond of the Tuskegee sewage treatment plant.        ;

                                      -11

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                                                                             4
                                                                             J
FIGUPvE 4.  Oral  papillona on the mouth fornix of a black bullhead.   X20.
                                        12

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                        Reproduced From
                        best  available copy.
FIGURE 5.   Superficial portion of an  oral  ^pillcras-  Epithelial cells,  goblet
cells, and  alarm substance cells are  arranged around lumens forming  cell nests
X60.
                                        13

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ANALYTICAL CHEMISTRY OF FIRA^ OXIDATION POND WATER

     Water collected on 16 November, 9 March 1980, 22 January  1982, and 3 March
1982 had unidentified nitrogen and  phosphorus organic residues  in the  100
ng/liter range.  No significant residues of pesticides, herbicides, or PCB were
detected in the water or sediment.  Water collected on 1 May 1981 contained
chloroform (9.0-13.5 ug/liter) and  bromodichloromethane (0.7 ug/liter), but
chlorodiibromcraethane and bronoform were not found with a detection limit of
1.0 ug/liter.  Chloroform concentrations were similar before chlorination and  ia
the final oxidation pond.


MUTAGENICITY OF THE FINAL OXIDATION POND WATER

     The acid fraction and the XAD  extract were mutagenic to Salmonella
typhimurium tester strains TA98 and TA100 only if S-9 (aroclor-induced rat liver
enzymes) was present.  The pmtagenicity of the organic extracts varied
seasonally (Fig. 6).  The basic fraction was cot mutagenic.  No differences have
been found between, extracts prepared by-organic extraction of  acidified water
and extracts prepared by filtering  the water through a resin column.  Water
samples collected at both the inlet and outlet of the final oxidation pond were
mutagenic, indicating that the mutagenicity is not lost during  retention in the
pond.


EXPOSURE OF FISH TO WATER IN THE  FINAL OXIDATION POND

     Papillomas developed on 5 of the black bullheads kept in  cages in the final
oxidation pond (Table 1).  The papillomas were located in the  same area of the
mouth and had the same gross and  histological appearance as the papillomas on
the wild black bullheads in the pond.  Four of the papillomas  developed between
467-537 days of exposure on fish  -in a sinking cage near the outlet.  One
papilloma developed in less than  57 days on a fish in a sinking cage at the
inlet B location.  The small namber of fish developing papillomas prevents
conclusions concerning the importance of cage location and contact with the
sediment.

     The most common types of lesions developing on  fish confined to cages in
the final oxidation pond were oral  mucosa hyperplasia and stomatitis usually
located in the mouth fornices.  The incidence of oral lesions  on caged fish in
the final oxidation pond varied depending on the fish species  and the  year that
the fish were exposed (Table 1).  The highest incidence was in black bullheads
stocked during October 1980 and the incidence was less in each  successive
stocking.  Black bullheads had the  highest prevalence of oral  lesions  of the A
species tested..  Similar oral lesions occurred on control black bullheads
(Table 1) but at a prevalence of  9% or less.  There  were no difference in
prevalence of hyperplasr.ir lesions  between floating  and sinking cages  or between
inlet and outlet locations.

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Table 1.  Maximum prevalence of oral  lesions  on caged  fish in the  final
          oxidation pond of the Tuskegee  sewage treatment  plant.   Control is the
          maximum prevalence of hyperplastic  oral  lesions  in caged fish  kept in
          a control pond.  Neoplasms  did  not  occur in  control fish.


Species         Stocking   Days of      Hyperplasia      Papillomas     Control
                  Date     Exposure     	     	   	
                                        %         N       %    N   days      %
black bullhead




21
23
29
9
8
Oct
Feb
Oct
Apr
Jul
80
81
81
82
82
168
43
407
245
57
95
50
33
25
17
22
12
6
8
12
80
0
0
0
8
5



12
537



57
4

0

9
yellow bullhead    12 May  81   683         0               0                14

brown bullhead     29 Oct  81   228         0               0                 0

channel catfish    16 Jan  81   436        30       10      0   '              8
                   29 Oct  81   513         4       28      0                 4
                    8 Jul  82   254         0               0                 5
                                       15

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          400
          3OO
         02OO
         "o
         u.
         v
         |
         z
           100
o-o-o Inlet 1982
»-e-« Outlet 1981
o     Outlet 1982
o	o Intel 1983
O     XAD -2
                          M
                    M    J    J    A
                      Months
                               *  -9
                                                       S    O
FIGURE 6.   Response of Salmonella  typhi.muri.um strain TA100 in the Ames  test  to
organic extracts  of water collected at  the  inlet .or outlet of the final
oxidation  pond  of the Tuskegee, Alabama,  sewage treatment plant.  The number of
colonies is  the difference between  test  and control plates.  The extracts  tested
were prepared by  solvent extraction of  acidified water samples or by XAD-2 resin
absorption.
                                       16

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INDUCTION OF HEPATIC ENZYME SYSTEMS

     UDP-GI in channel catfish ire the final  oxidation pond was higher than in
control channel catfish (Fig. 7).  UDP-GT activity  in other  ictalurid species
and ST activity in all species tested in the  final  oxidation pond were not
consistently different than controls.
VIROIOGY OF THE PAPILLOMAS

     Examination of papillomaa with TEM  failed  to  reveal virus-like structures.
Fish injected with homogenised papillomas were  observed  11-14 months without
signs of papilloaas or hyerplastic lesions.


EXPOSURE OF BROWN BULLHEAD EMBROYS TO FINAL OXIDATION  POND WATER AND AFB

     Trunk kidneys of fish, 25 days after exposure to  1.0 mg/liter AFB, had
atrophied glomeruli and renal tublar necrosis.  Focal  areas  of  atrophied
epithelial cells of renal tubules were dispersed among tubules  of normal
structure.  Livers of fish with- renal lesions appeared normal.

     Twelve fish from the embryo exposure to  1.0 mg/liter AFB were examined
after eight months.  Pathological effects were  absent  in all liver and kidney
tissue examined.

     Exposure of brown bullhead embryos  to 0.5  mg/liter AFB  did not cause
pathological effects to livers and trunk kidneys at any development stage
examined.  Liver tissue from a subsample of this group showed normal
ultrastructure, with individual variation in  glycogen  content.

     No pathological effects were observed in livers or  trunk kidneys of brown
bullheads 25 days after embryo exposure  to an organic  concentrate of Tuskegee
effluent water.
LABORATORY EXPOSURES OF  BLACK  BULLHEADS  TO  SEDIMENT  EXTRACTS

     Black bullheads injected  with  0.1 ml DMSO developed  necrosis  at  the
injection site.  Bacterial  infections occurred in  the  black bullheads being
swabbed with sediment extract.  No  tumors developed  in either  the  injected-or
swabbed fish after 8. months.
                                       17

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                12
                 9
                 8
             Q,
                 4
                 3
                 2
                 1
                          -E--
                          -C
- exposed
- control
                     Dec 81 Feb82 Apr 82 Jun82
                                     6AfE
                      Nov82
FIG 7.  UDP-glucuronosyltransferase (UDP-GT)  activity (nmol/min/mg protein)  in
liver Dvicrosoraes  of caged channel catfish in  the  final" oxidation poad cf the
Tuskegee, Alabama, sewage treatment plant or  in a control pond.
                                     18

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                                    SECTION  6

                                    DISCUSSION
     Histologically,  the black  bullhead  papillomas  were similar  to those  of
brown bullheads  Ictalurus nebulosus  described  by Lucke  and Schlumberger  (1941),
Harshbarger (1977) considered bullhead papillomas to  be a common type of  fish
neoplasm.  However the papillomas  in the present case are distinctive because
most were uniformly  located  in  the mouth fornices rather than in variable
locations.

     The neoplastic  nature of the  papillomas we described is indicated not only
by the histopathology but also  by  their  persistence after removal of the  fish
from the final oxidation pond.   If these lesions were inflammatory responses
they would have  regressed more  quickly.

     The reason- for  the uniform location of the papillomas in this population  of
black bullheads  may  be related  to  the presence of the oral valve in the  anterior
buccal cavity.   The  oral valve  is  a  thin fold  of mucosa located  immediately
posterior to the upper and lower lips.   The folds forming the oral valve
terminate laterally  near the mouth fornix,  and the  lateral ends  of these  folds
were often inflammed  in fish, including  controls, kept  in cages  during this
study.  The high incidence of mucosal hyperplasia in  the oral valve area  also
indicates that this  location is sensitive to  toxicants.

     No evidence was  found that a  virus  was associated  with the, papiliomas of
black bullheads. This is in contrast to other fish papillomas in which  viruses
can be seen in electron micrographs  (Edwards  et al. 1977) or isolated in  cell
culture (Schw&nz-Pfitzner 1976).  If a virus  is associated with  the black
bullhead papillo-nas,  they are unlike those  .previously reported to be present in
fish .papillomas.

     In contrast to  the direct-acting mutagens pre'sent  in the neutral or  basic
fraction of wastewater from  other  sewage treatment  plants (Saxena and Schwartz
1979, Rappaport. et al. 1979, Gumming et  al. 1980),  the  aciJic fraction of the
Tuskegee sewage  'effluent was most  uutagenic but only  after metabolic activation
by S-9.  This indicates that the primary mutagen in the Tuskagee wastewater is
different than in previously reported cases of mutagenic wastewater.  Both the
activated sludge process (Rappaport  et  al.  1979) and  disinfection with chlorine
(Cunnaing et al.  1980) have been implicated  in  increasing mutagenicity; both of
these factors could  be  involved .in the  present case.

     The cause of seasonal changes in mutagenicity of the Tuskegee wastewater  is
unknown but may  be related  to higher temperatures during chlorination because
the pe?k mutagenicity is during summer.   Seasonal variation in wastewater
contaminants such as pesticides could also  be  involved.  Accumulation or  organic
material  in filter beds of  treatment plants was suggested as a cause of  seasonal
variation in mutagenicity of drinking water (Grimm-Kibalo 1981)".  Variation in
domestic wastewater  mutagenicity could  be related to  variation in drinking water
mutagenicity.                               .        .                       ;,


                                       19 .

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     The induction of UDP-GT in channel  catfish  confined  to  the  final  oxidation
pond indicates exposure to a toxicnt.  Similar induction  occurs  in  rats  and  fish
given oral or intraperitoneal doses of carcinogens.  The  seasonal ch&nges  in
UDF-GT activity also strongly indicates  the effect of  temperature on enzyme
induction in fish.  The conjugase-enzyme induction in  channel  catfish  but  not  in
black-bullheads may be related to the greater susceptibility of  black  bullheads
to the tumor inducing effects of chemical  carcinogens  in  the final  oxidaiton
pond.

     The usefulness of exposing caged fish to water  for detection of chemical
carcinogens was demonstrated by the development  of neoplasms on  caged  black
bullheads.  The use of chemical analysis in  this case  failed to  indicate that
mutagenic or carcinogenic chemicals were present.  Laboratory  exposures  of black
bullheads and brown billhead embryos to organic extracts of the Tuskegee
wastewater failed to cause tumors.  Additional refinement of techniques  may
improve the usefulness of laboratory exposures,  but  presently  field exposures
of caged fish are more conclusive.

     The role of chlorine in causing the black bullhead papillomas  was indicated
by the reduced prevalence of tumore after  the chlorination rate  was reduced.
Additional study of the Tuskegee, Alabama, sewage treatment  plant  is warranted
to determine the identity of the carcinogenic chemicals and  the  relationship
between chlorination and tumors.
                                       20

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                                      22

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